CN110846024A - Near-infrared multiband photoelectric response up-conversion @ MoS2Composite material and use thereof - Google Patents

Near-infrared multiband photoelectric response up-conversion @ MoS2Composite material and use thereof Download PDF

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CN110846024A
CN110846024A CN201911132259.0A CN201911132259A CN110846024A CN 110846024 A CN110846024 A CN 110846024A CN 201911132259 A CN201911132259 A CN 201911132259A CN 110846024 A CN110846024 A CN 110846024A
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mos
conversion
composite material
upconversion
rare earth
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高潮
吴玲
黄一波
王乾
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Changzhou Vocational Institute of Engineering
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    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
    • C09K11/68—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals containing chromium, molybdenum or tungsten
    • C09K11/681—Chalcogenides
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    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
    • C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
    • C09K11/7772—Halogenides
    • C09K11/7773—Halogenides with alkali or alkaline earth metal

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Abstract

The invention discloses near-infrared multiband photoelectric response up-conversion @ MoS2The composite material has a core-shell structure, wherein the up-conversion micrometer rod material is used as a core, and MoS is adopted2The shell is made of an up-conversion micrometer rod material NaYF4The up-conversion micrometer rod material is doped with one or more rare earth metal ions, wherein the molar percentage of the rare earth metal ions in the composite material is 0.1-90 mol%. Up-conversion @ MoS of the invention2Upconversion micrometer rod material in composite materialHas stronger absorption capability to near infrared light within the range of 950-1600 nm, solves the problem of MoS2The response to near infrared light is weak.

Description

Near-infrared multiband photoelectric response up-conversion @ MoS2Composite material and use thereof
Technical Field
The invention belongs to the technical field of material chemistry, and particularly relates to near-infrared multiband lightElectric response up-conversion @ MoS2Composite materials and their use.
Background
In recent years, molybdenum disulfide (MoS)2) As a representative two-dimensional transition metal sulfide, a wide research interest has been raised. MoS2The graphene has a layered structure similar to graphene, and has the characteristics of high carrier mobility and the like. Unlike graphene, MoS2Has adjustable band gap, and is suitable for use as efficient photoelectric detector. Research shows that MoS2The band gap of (a) is related to the number of layers, MoS as the number of layers decreases2The band gap of (A) varies in the range of 1.2eV to 1.8 eV. Nevertheless, due to the limitation of the band gap range, MoS2Typically in the visible range of wavelengths less than 1000 nm. Thus, how to implement and enhance MoS2The near infrared band detection of (2) is a hot research subject.
In previous studies, researchers have proposed using layered composite structures to promote MoS2Near infrared response of (c). Kufer et al reported 2014 that PbS quantum dot and MoS2The PbS quantum dots can absorb near infrared light of more than 1000nm, and they will MoS2And PbS quantum dots are loaded on the channel of the field effect transistor in the form of thin films respectively, so that the enhancement of near-infrared photoelectric response is realized (adv. Mater.27(1) (2015) 176-180); same composite structure adopted by Zhou et al in 2017 to promote MoS2Near infrared photoelectric response of (1), NaYF they use4:Yb/Er@NaYF4Nd/Yb nanoparticles can absorb excitation light at 808nm and 980nm in a narrow band (J.Mater.chem.C5(7) (2017) 1591-. The method for obtaining the composite structure is to make the near-infrared absorbing material and the molybdenum sulfide in layered physical contact, and the distance between the near-infrared absorbing material and the molybdenum sulfide is too large, so that the energy transfer efficiency between the near-infrared absorbing material and the molybdenum sulfide is very low, and the photoelectric response capability of the composite structure needs to be further improved. Up-conversion @ MoS with core-shell structure has not been provided so far2The composite material is applied to relevant reports on near-infrared multiband photoelectric response.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a near-infrared multiband photoelectric response up-conversion @ MoS2Composite material and application thereof, up-conversion @ MoS2The composite material utilizes the upconversion micrometer rod material to have stronger absorption capacity on near infrared light within the range of 950-1600 nm, and solves the problem of MoS2The response to near infrared light is weak.
The technical scheme of the invention is to provide near-infrared multiband photoelectric response up-conversion @ MoS2The composite material has a core-shell structure, wherein the up-conversion micrometer rod material is used as a core, and the MoS is2The shell is made of an up-conversion micrometer rod material NaYF4The up-conversion micrometer rod material is doped with one or more rare earth metal ions, wherein the molar percentage of the rare earth metal ions in the composite material is 0.1-90 mol%.
The preferable technical scheme is that the up-conversion micrometer rod material is hexagonal phase NaYF4。
In a preferred technical scheme, the rare earth metal salt is Yb3+/Er3+、Yb3+/Ho3+、Yb3+/Tm3+、Er3+、Er3 +/Tm3+Or Er3+/Ho3+Wherein Yb is3+The mole percentage of ions in the composite material is 5-90 mol%, and Er3+The mole percentage of ions in the composite material is 0.2-5 mol%, Ho3+The mole percentage of ions in the composite material is 0.2-5 mol%, and Tm3+The mole percentage of the ions in the composite material is 0.1-5 mol%.
According to a further preferable technical scheme, the rare earth metal salt adopted as the raw material for preparing the up-conversion micron rod material is rare earth nitrate or rare earth chloride.
To facilitate this near-infrared multiband photoelectric response upconversion @ MoS2The application and implementation of the composite material provide a near-infrared multiband photoelectric response up-conversion @ MoS2CompoundingUse of a material, converting said up-conversion @ MoS2The composite material is used as a near infrared light responsive matrix.
The preferred technical scheme is that the up-conversion @ MoS2The wavelength range of the near infrared light responded by the composite material is 950-1600 nm.
The invention has the advantages and beneficial effects that:
the invention provides up-conversion @ MoS of near-infrared multiband photoelectric response2Composite material, the upconversion @ MoS2The composite material has a core-shell structure, wherein the up-conversion micrometer rod material is used as a core, and the MoS is2To the shell, the upconversion @ MoS2The composite material can generate photoelectric response to near infrared light within the range of 950-1600 nm.
Drawings
FIG. 1 is NaYF in example 14Scanning electron microscope images of Yb/Er micron rods;
FIG. 2 shows NaYF in example 14:Yb/Er@MoS2Transmission electron micrographs of the composite;
FIG. 3 shows NaYF in example 14:Yb/Er@MoS2Photoelectric response characterization (I-t curve) of the composite material under 980nm laser excitation;
FIG. 4 shows NaYF in example 24A scanning electron microscope image of an Er micron rod;
FIG. 5 shows NaYF in example 24:Er@MoS2Transmission electron micrographs of the composite;
FIG. 6 shows NaYF in example 24:Er@MoS2And the photoelectric response of the composite material under the excitation of 1532nm laser is characterized (I-t curve).
Detailed Description
The following description of the embodiments of the present invention will be made with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
Up-conversion @ MoS of near-infrared multiband photoelectric response2The synthesis method of the composite material comprises the following steps:
s1: preparing up-conversion micrometer rod materials doped with different rare earth ions by using a liquid phase method;
s2: pretreating the up-conversion micrometer rod material prepared in the step S1 to remove surface ligands, and dispersing the material in an aqueous solution;
s3: uniformly mixing and dispersing the up-conversion micrometer rod material with the surface ligand removed in the step S2, ammonium tetrathiomolybdate and disodium ethylene diamine tetraacetate into an aqueous solution to obtain a reactant mixed solution;
s4: and (4) carrying out hydrothermal reaction on the reactant mixed liquor prepared in the step (S3), and washing and centrifuging the reaction product after the hydrothermal reaction is finished to obtain the target product.
Example 1
S1: solvothermal synthesis of NaYF4The Yb/Er (18/2 mol%) micron rod is synthesized by the following steps: adding 5mL of ethanol and 5mL of oleic acid into 1.5mL (7.5mmol) of sodium hydroxide aqueous solution, and stirring for 40 min; adding 1mL of 2mol/L fluorinated ammonia water solution, and continuing stirring for 40 min; adding 1.6mL of 0.2mol/L yttrium nitrate aqueous solution, 0.36mL of 0.2mol/L ytterbium nitrate aqueous solution and 0.04mL of 0.2mol/L erbium nitrate aqueous solution into the solution, and continuously stirring for 1h to obtain reactant mixed solution; transferring the reactant mixed solution into a 20L polytetrafluoroethylene reaction kettle, reacting at 220 ℃ for 12h, cooling to room temperature, washing the reaction solution with ethanol and water, centrifuging for 3 times, dispersing the obtained white upconversion micrometer rod material into 4mL of ethanol for later use, wherein a scanning electron microscope image of the upconversion micrometer rod material is shown in FIG. 1;
s2: the upconversion micrometer rod material synthesized in an oleic acid system is hydrophobic, and in order to enable the upconversion micrometer rod material to be a hydrophilic material, HCl is used for removing oleic acid ligands on the surface, and the specific steps are as follows: taking 1mL of 0.1mol/L NaYF4Putting an ethanol solution of Yb/Er into a 2mL centrifuge tube, and putting the centrifuge tube into a centrifuge for 1min at 12000 rpm; dispersing the lower layer precipitate in 750 μ L ethanol for ultrasonic treatment, adding 500 μ L1 mol/L dilute hydrochloric acid for continuous ultrasonic treatment for 30s after uniform dispersion, then placing the centrifuge tube in a centrifuge for 15min at 12000rpm, pouring out the upper layer solution, dispersing the lower layer precipitate in 750 μ L ethanol for ultrasonic treatment, adding 50 μ L1 mol/L dilute hydrochloric acid for continuous ultrasonic treatment for 10s after uniform dispersionCentrifugation at 12000rpm for 15min, and dispersion of the centrifuged white precipitate in 0.5mL of H2O for later use;
s3: adding 1mL of 0.2mol/L NaYF for washing oleic acid ligand into 4mL of 0.04mmol of ethylene diamine tetraacetic acid disodium aqueous solution and 4mL of 0.2mmol of sodium fluoride aqueous solution4Stirring Yb/Er water solution for 40 min; then adding 6mL of 0.2mmol ammonium tetrathiomolybdate aqueous solution, and continuing stirring for 1h to obtain reactant mixed liquor;
s4: transferring the reactant mixed solution into a 20mL reaction kettle, reacting at 220 ℃ for 12h, and cooling to room temperature to obtain a reaction product mixed solution; washing the reaction product mixture with ethanol and water, and centrifuging for 3 times to obtain NaYF4:Yb/Er@MoS2Composite material, NaYF4:Yb/Er@MoS2Transmission electron microscopy of the composite see FIG. 2, NaYF4:Yb/Er@MoS2The photoelectric response of the composite material under the excitation of 980nm laser (I-t curve) is characterized in figure 3.
Example 2
S1: solvothermal synthesis of NaYF4Er (2 mol%) micron rod, the synthesis steps are as follows: adding 5mL of ethanol and 5mL of oleic acid into 1.5mL (7.5mmol) of sodium hydroxide aqueous solution, and stirring for 40 min; adding 1mL of 2mol/L fluorinated ammonia water solution, and continuing stirring for 40 min; adding 1.96mL of 0.2mol/L yttrium nitrate aqueous solution and 0.04mL of 0.2mol/L erbium nitrate aqueous solution into the solution, and continuously stirring for 1h to obtain reactant mixed solution; transferring the reactant mixed solution into a 20L polytetrafluoroethylene reaction kettle, reacting at 220 ℃ for 12h, cooling to room temperature, washing the reaction solution with ethanol and water, centrifuging for 3 times, and dispersing the obtained white upconversion micrometer rod material into 4mL of ethanol for later use, wherein a scanning electron microscope image of the upconversion micrometer rod material is shown in a figure 4;
s2: the upconversion micrometer rod material synthesized in an oleic acid system is hydrophobic, and in order to enable the upconversion micrometer rod material to be a hydrophilic material, HCl is used for removing oleic acid ligands on the surface, and the specific steps are as follows: taking 1mL of 0.1mol/L NaYF4Placing the Er ethanol solution in a 2mL centrifuge tube, and placing the centrifuge tube in a centrifuge for 1min at 12000 rpm; dispersing the lower layer precipitate in 750 μ L ethanol for ultrasonic treatment,adding 500 mu L of 1mol/L dilute hydrochloric acid after uniform dispersion, continuing to perform ultrasonic treatment for 30s, then placing the centrifugal tube into a centrifugal machine, centrifuging at 12000rpm for 15min, pouring out the upper layer solution, dispersing the lower layer precipitate in 750 mu L ethanol for ultrasonic treatment, adding 50 mu L of 1mol/L dilute hydrochloric acid after uniform dispersion, continuing to perform ultrasonic treatment for 10s, centrifuging at 12000rpm for 15min, dispersing the white precipitate obtained by centrifugation in 0.5mL H2O for later use;
s3: adding 1mL of 0.2mol/L NaYF for washing oleic acid ligand into 4mL of 0.04mmol of ethylene diamine tetraacetic acid disodium aqueous solution and 4mL of 0.2mmol of sodium fluoride aqueous solution4Stirring Er aqueous solution for 40 min; then adding 6mL of 0.2mmol ammonium tetrathiomolybdate aqueous solution, and continuing stirring for 1h to obtain reactant mixed liquor;
s4: transferring the reactant mixed solution into a 20mL reaction kettle, reacting at 220 ℃ for 12h, and cooling to room temperature to obtain a reaction product mixed solution; washing the reaction product mixture with ethanol and water, and centrifuging for 3 times to obtain NaYF4:Yb/Er@MoS2Composite material, NaYF4:Yb/Er@MoS2Transmission electron microscopy of the composite see FIG. 5, NaYF4:Yb/Er@MoS2The photoelectric response of the composite material under 1532nm laser excitation (I-t curve) is characterized in FIG. 6.
FIGS. 3 and 6 show the upconversion @ MoS of the near infrared multiband photoelectric response prepared in examples 1 and 22The composite material generates photoelectric response to near infrared light within the range of 950-1600 nm, and the aim of the invention is achieved.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the technical principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (6)

1. Near-infrared multiband photoelectric response up-conversion @ MoS2The composite material has a core-shell structure, wherein the up-conversion micrometer rod material is used as a core, and the MoS is2Is a shell, and is characterized in that the up-conversion micrometer rod material is NaYF4Said upconversion micronThe rod material is doped with one or more rare earth metal ions, wherein the molar percentage of the rare earth metal ions in the composite material is 0.1-90 mol%.
2. The near-infrared multiband photoelectric response upconversion @ MoS of claim 12The composite material is characterized in that the up-conversion micrometer rod material is hexagonal phase NaYF4。
3. The near-infrared multiband photoelectric response upconversion @ MoS of claim 1 or 22The composite material is characterized in that the rare earth metal ion is Yb3+/Er3+、Yb3+/Ho3+、Yb3+/Tm3+、Er3+、Er3+/Tm3+Or Er3+/Ho3+Wherein Yb is3+The mole percentage of ions in the composite material is 5-90 mol%, and Er3+The mole percentage of ions in the composite material is 0.2-5 mol%, Ho3+The mole percentage of ions in the composite material is 0.2-5 mol%, and Tm3+The mole percentage of the ions in the composite material is 0.1-5 mol%.
4. The near-infrared multiband electro-optic response up-conversion @ MoS of claim 32The composite material is characterized in that the rare earth metal salt adopted as the raw material for preparing the up-conversion micron rod material is rare earth nitrate or rare earth chloride.
5. The near-infrared multiband photoelectric response upconversion @ MoS of claim 12Use of a composite material, characterized in that the upconversion @ MoS is performed2The composite material is used as a near infrared light response.
6. The near-infrared multiband electro-optic response up-conversion @ MoS of claim 52Use of a composite material, characterized in that the upconversion @ MoS2The wavelength range of the near infrared light responded by the composite material is 950-1600 nm.
CN201911132259.0A 2019-11-19 2019-11-19 Near-infrared multiband photoelectric response up-conversion @ MoS2Composite material and use thereof Pending CN110846024A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104371725A (en) * 2014-10-27 2015-02-25 肖思 Preparation method of NaYF4:Yb/Er-MoS2 conjugate
CN105219390A (en) * 2015-09-08 2016-01-06 兰州大学 A kind of upper converting material, preparation method that can be applicable to dye sensitization solar battery
CN110255619A (en) * 2019-06-21 2019-09-20 南京工业大学 A method of based on upper conversion nano particle preparation three-dimensional hollow structure molybdenum sulfide
CN110358538A (en) * 2019-07-22 2019-10-22 西安建筑科技大学 A kind of NaYF4:Yb3+/Ln3+Micron bar array structure and preparation method thereof
CN110420652A (en) * 2019-08-14 2019-11-08 哈尔滨工业大学 A kind of NaYF4:Yb/Er@MoS2Core-shell structure micron crystalline substance and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104371725A (en) * 2014-10-27 2015-02-25 肖思 Preparation method of NaYF4:Yb/Er-MoS2 conjugate
CN105219390A (en) * 2015-09-08 2016-01-06 兰州大学 A kind of upper converting material, preparation method that can be applicable to dye sensitization solar battery
CN110255619A (en) * 2019-06-21 2019-09-20 南京工业大学 A method of based on upper conversion nano particle preparation three-dimensional hollow structure molybdenum sulfide
CN110358538A (en) * 2019-07-22 2019-10-22 西安建筑科技大学 A kind of NaYF4:Yb3+/Ln3+Micron bar array structure and preparation method thereof
CN110420652A (en) * 2019-08-14 2019-11-08 哈尔滨工业大学 A kind of NaYF4:Yb/Er@MoS2Core-shell structure micron crystalline substance and preparation method thereof

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Application publication date: 20200228